EP3589773B1 - Cible de pulvérisation et procédé de production d'une cible de pulvérisation - Google Patents

Cible de pulvérisation et procédé de production d'une cible de pulvérisation Download PDF

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EP3589773B1
EP3589773B1 EP18706710.3A EP18706710A EP3589773B1 EP 3589773 B1 EP3589773 B1 EP 3589773B1 EP 18706710 A EP18706710 A EP 18706710A EP 3589773 B1 EP3589773 B1 EP 3589773B1
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target
elements
equal
powder
group
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EP3589773A1 (fr
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Peter Polcik
Szilard KOLOZSVARI
Paul MAYRHOFER
Helmut Riedl
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Plansee Composite Materials GmbH
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Plansee Composite Materials GmbH
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
    • C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
    • C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3411—Constructional aspects of the reactor
    • H01J37/3414—Targets
    • H01J37/3426—Material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B22F2301/205—Titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides

Definitions

  • the present invention relates to a target for use in a physical vapor deposition process with the features of the preamble of claim 1, a method for powder metallurgical production of a target which is intended for use in a physical vapor deposition process and the use of such a target in a physical vapor deposition process .
  • Various methods are available for physical vapor deposition, e.g. B. evaporation, sputtering (sputter deposition) or arc evaporation (cathodic arc deposition or arc-source evaporation technique).
  • a target is suitable for use in a PVD process for depositing layers on a substrate material provided for this purpose.
  • target is to be understood in particular as meaning sputtering targets and targets for arc vaporization (also called arc cathodes).
  • the targets are manufactured using different technologies.
  • powder metallurgy processes There are many different options in powder metallurgy processes, which must be selected according to the composition of the target, taking into account the properties of the integrated elements. Examples here are pressing, sintering, hot isostatic pressing (HIP), Forging, rolling, hot pressing (HP) or spark plasma sintering (SPS) - also in combination with each other.
  • the targets also called coating sources or sources for short
  • the targets are thermally impacted by the plasma, the arc and last but not least by the heating in the coating chamber. In order to avoid excessive heating of the coating sources, they are cooled from the rear. This cooling can be done either via direct water cooling of the back of the target or via indirect cooling via a rigid copper backplate or flexible copper membranes.
  • the CN104480444 describes a target composition with Ti from 10 - 50 at%, Al from 40 - 90 at%, and contents of Co, Cr, Ta, W, Nb, Mo, Zr, V, B, Si, Y, La, Se and Ce, with Co 0.1 - 10 at%, Cr 0.1 - 20 at%, Ta 0.1 - 10 at%, W 0.1 - 10 at%, Nb 0.1 - 10 at%, Mo 0.1 - 10 at%, Zr 0.1 - 10 at%, V 0.1 - 10 at%, B 0.1 - 10 at%, Si 0.1 - 20 at%, Y 0.1 - 10 at%, La 0.01 - 5 at%, Ce 0.01 - 5 at%, Se 0.01 - 5 at% .
  • the JPH08151269A is directed to a thermoelectric material based on iron, a lanthanide and silicon
  • composition of the target itself also has a major influence on the coating rate.
  • the existing bonds define how much impact energy (especially during sputtering) is necessary to convert an atom or cluster of atoms from the target surface into the gas phase.
  • the working gas Ar is given below as an example for the working gas, this is not intended to be a limitation
  • secondary electrons are also produced, which in turn result in more Ar ions being produced, which can sputter more atoms of the target.
  • the effectiveness of these sputtering processes depends very much on the energy introduced and, above all, on the energy density. The target can only be sputtered when this is high enough.
  • the coating rate also atomization rate, sputtering rate
  • the energy density can be increased by higher energies of the arriving Ar ions or by other parameters of the coating systems (such as magnetic fields, which increase the interaction of the secondary electrons with the working gas and thus its degree of ionization). Mainly due to a higher energy of the Ar ions hitting it but also the thermal load on the targets (nearly 90% of the impacting energy of the Ar ions is converted into heat and only a small percentage is used for the desired sputtering). Essentially, these are all process-controlled parameters.
  • the object of the invention is to provide a target and a method for producing targets in which there is an increased evaporation rate and thus an increased coating rate.
  • the essential advantage of the invention lies in an increased coating rate (and thus faster layer growth), which can be achieved by relatively low doping of the target with the selected elements from the group of lanthanides: La, Ce, Nd, Sm and Eu.
  • the invention is based on the applicant's finding that the coating rate can be influenced very effectively by adding doping elements. This is essentially based on two effects: On the one hand, the selected doping elements from the group of lanthanides: La, Ce, Nd, Sm and Eu, help to use the available energy of the Ar ions more effectively with regard to the spatial expansion of the interaction area. Due to their size and mass, the selected doping elements act like atomic "battering rams" (if they are distributed homogeneously in the target, as is the case with targets produced by powder metallurgy), which concentrate the existing impact energy or impulse on a smaller interaction area on the target surface .
  • the selected doping elements from the group of lanthanides: La, Ce, Nd, Sm and Eu, help to use the available energy of the Ar ions more effectively with regard to the spatial expansion of the interaction area. Due to their size and mass, the selected doping elements act like atomic "battering rams" (if they are distributed homogeneously in the target, as
  • the transferred kinetic energy is concentrated in fewer atomic layers and the total energy of the impinging Ar ions can be concentrated in a smaller area.
  • This increases the sputtering rate with constant energy of the impinging Ar ions and a more efficient sputtering process occurs. This is accompanied by an increase in the secondary electron emission, which in turn leads to a higher degree of ionization of the working gas.
  • the secondary electron emission can also be increased by the selected doping elements from the group of lanthanides: La, Ce, Nd, Sm and Eu, which have a particularly low electron work function.
  • a lower electron work function means an increased number of secondary electrons and thus an increased probability of the formation of ions in the working gas, which in turn can eject more target atoms.
  • Another positive effect in reactive sputtering processes is that poisoning of the target surface is more difficult due to the increased energy density (in the more concentrated near-surface interaction areas of the target due to the corresponding elements).
  • the formation of poorly electrically conductive reaction products of the target with the reactive gas (e.g. N2) and their retention on the target surface (which leads to the well-known poisoning of the target) is made more difficult. If such products form, they are immediately removed again by the increased number of Ar ions present, and the target thus remains in the desired metallic sputtering mode longer (even with higher N2 proportions in the atmosphere).
  • the reactive gas e.g. N2
  • the positive effect of the invention lies above all in the increased electron density on the target surface, which in turn increases the arc events and thus the evaporation rate.
  • the selected elements from the group of lanthanides: La, Ce, Nd, Sm and Eu also have a positive influence on the layer properties in terms of the achievable hardness or wear resistance.
  • the doping elements are introduced into the targets in the form of ceramic compounds or, according to a variant not according to the invention, alternatively in the form of aluminum alloys in order to be able to ensure low oxygen contents in the target:
  • the elements listed here have a high chemical affinity for oxygen and therefore oxidize very quickly in pure metallic or unalloyed form. If the doping elements were in the form of oxides, they would not be electrically conductive and would therefore be very difficult to convert into the vapor phase in the deposition process.
  • ceramic compounds such as borides, carbides, nitrides and silicides or Al-based alloys, these elements are largely protected from oxidation.
  • Cerium disilicide is particularly suitable for adding cerium, as it is much more resistant to oxidation in the target production temperature range (up to 350°C) compared to metallic cerium.
  • cerium disilicide is very brittle, which means that particularly fine-grained powders can be produced by mechanical comminution (milling). This is favorable for the powder metallurgical production of the targets. A particularly homogeneous distribution of the doping element is achieved with fine-grained powders.
  • An oxygen content in the target below 5000 ⁇ g/g, preferably below 3000 ⁇ g/g, is also found to be particularly favorable for the layer properties.
  • high levels of oxygen lead to a weakening of the strength of grain boundaries (softening of the interfaces), which in turn leads to a reduction in the hardness and the modulus of elasticity of the layers.
  • a large difference in the work functions of the elements that make up the target can also mean that the different grains that make up the structure of the target z.
  • figure 1 shows the coating rate in nm/min as a function of the content y [at.%] of the doping elements Ce or La for a TiAl, TiAlCe, and TiAILaB6 target.
  • the deposition rate was determined by SEM in cross-sectional configuration for Ti 1-x Al x N, Ti 1-xy Al x Ce y N, and Ti 1-xy Al x (LaB 6 ) y N layers.
  • the coating rate for the undoped TiAl target corresponds to the point with 0 at.% doping element.
  • the contents y of the doping elements Ce and La were determined in the deposited layer, the molecular formula for the composition of the layer is Ti 1-xy Al x (Ce/La) y N.
  • the concentrations of the elements in the layer were determined by EDX.
  • Targeted alloying of the targets with approx. 2 to 2.5 at% enabled the sputtering rate to be increased by 50 to 80% for reactive sputtering (gas mixture: Ar/N2).
  • the lanthanum is present in the target as LaB6, but in the layer deposited from it as elemental lanthanum—preferably on lattice sites of Ti or Al—is present.
  • figure 2 shows a light micrograph of a TiAILaB6 target in cross section. As marked in the picture, the light areas are made of aluminum, the gray areas are made of titanium and the black areas are made of LaB6 powder particles.
  • figure 3 shows a light micrograph of a TiAlCe target in cross section.
  • the light areas are made of aluminum
  • the gray areas are made of titanium powder particles
  • the fine-grained dark gray agglomerates are made of a CeAl alloy.
  • the black areas in the structure correspond to cavities caused by the preparation (breakouts when the sample was ground).
  • the powder batch was then forged at room temperature to form a compact and then at 350° C. to form a blank.
  • a target with dimensions of ⁇ 75 x 6 mm was machined from the blank by mechanical machining.
  • the nature of such a material is figure 2 shown, using a light micrograph of a cross section of the material.
  • the targets produced in this way, disks with the dimensions ⁇ 75 x 6 mm, were then bonded to copper cathodes of a laboratory coating system (adapted Leybold Heraeus Z400) using indium and installed in the system. in one In the PVD process, the targets were sputtered at a total pressure of 0.35 Pa in a gas mixture of Ar and N 2 (20% N 2 content).
  • the targets were operated at a power density of 9.0 W/cm 2 for a period of 35 minutes.
  • the resulting layers were deposited on monocrystalline Si flakes (100 orientation, 20x7x0.38 mm 3 ) and metallographically polished austenite flakes (20x7x0.8 mm 3 ).
  • the substrate materials were cleaned in acetone and ethanol before being thermally etched in the coating system at 430 ⁇ 20 °C. Subsequent to this thermal etching process, plasma etching was also carried out in a pure Ar atmosphere at a total pressure of 6 Pa (duration 10 min). During the coating process, the substrate temperature was 430 ⁇ 20 °C, the bias potential was -50 V.
  • the layers deposited in this way have a very dense morphology and a face-centered cubic crystal structure, which was determined using scanning electron microscopy (SEM) and X-ray diffraction (XRD). was investigated.
  • the chemical composition was determined using energy-dispersive X-ray spectroscopy (EDX) in the SEM.
  • EDX energy-dispersive X-ray spectroscopy
  • the thickness of the layers was approx. 3650 and 4800 nm (the 3650 nm were achieved for the layer with approx. 1.5 at% La in the layer), for the respective La contents ( figure 1 ).
  • the mechanical properties of the Ti 1-xy Al x La y N layers were tested by nanoindentation and showed an increase compared to pure Ti 1-x Al x N deposited under the same conditions.
  • the powder batch was then forged at room temperature to form a compact and then at 350° C. to form a blank.
  • a target with dimensions of ⁇ 75 x 6 mm was machined from the blank by mechanical machining.
  • the nature of such a material is figure 3 shown, using a light micrograph of a cross section of the material.
  • the targets produced in this way, with the dimensions ⁇ 75 x 6 mm, were then bonded to copper cathodes of a laboratory coating system (adapted Leybold Heraeus Z400) using indium and installed in the system.
  • the targets were sputtered at a total pressure of 0.35 Pa in a gas mixture of Ar and N 2 (20% N 2 proportion).
  • the targets were operated at a power density of 9.0 W/cm 2 for a period of 45 min.
  • the resulting layers were deposited on monocrystalline Si flakes (100 orientation, 20x7x0.38 mm 3 ) and metallographically polished austenite flakes (20x7x0.8 mm 3 ).
  • the substrate materials were cleaned in acetone and ethanol before being thermally etched in the coating system at 430 ⁇ 20 °C.
  • plasma etching was also carried out in a pure Ar atmosphere at a total pressure of 6 Pa (duration 10 min).
  • the substrate temperature was 430 ⁇ 20 °C.
  • the bias potential was -50 V.
  • the layers deposited in this way have a very dense morphology and a face-centered cubic crystal structure, which was examined by means of scanning electron microscopy (SEM) and X-ray diffractometry (XRD).
  • the chemical composition was determined using energy-dispersive X-ray spectroscopy (EDX) in the SEM.
  • the layers have thicknesses of approx. 3600 and 5000 nm. These two different layer thicknesses were obtained by placing 8 pieces of TiAl (4x4x4 mm 3 , chemical composition of Ti/Al 50/50 at%) in the racetrack to reduce the Ce content, thus reducing the amplification of the coating rate .
  • the powder batch was then forged at room temperature to form a compact and then at 350° C. to form a blank. Finally, a target with dimensions of ⁇ 75 x 6 mm was machined from the blank by mechanical machining.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)

Claims (8)

  1. Cible pour l'utilisation dans un processus de dépôt physique en phase vapeur, comportant une matrice composée d'un matériau composite choisi dans le groupe constitué par un matériau à base d'aluminium, un matériau à base de titane ainsi que de quelconques combinaisons correspondantes, les éléments de la matrice formant une proportion supérieure ou égale à 60 % at et inférieure ou égale à 99 % at de la cible, la matrice étant dopée avec des éléments de dopage, les éléments de dopage étant choisis dans le groupe des lanthanoïdes : La, Ce, Nd, Sm et Eu, caractérisée en ce que les éléments de dopage sont incorporés en tant qu'ingrédients de composés céramiques dans la matrice et en ce que les éléments de dopage sont présents au total en une concentration dans la cible dans une plage de supérieur ou égal à 1 % at et inférieur ou égal à 10 % at, de préférence inférieur ou égal à 5 % at.
  2. Cible selon la revendication 1, la matrice étant présente en tant que matériau à base d'aluminium dans une composition de AlxM1-x, M étant un ou plusieurs éléments du groupe de Ti, V, Cr, Zr, Nb, Mo, Ta, W, Si et x étant supérieur à 25 % at.
  3. Cible selon au moins l'une quelconque des revendications précédentes, la teneur en oxygène dans la cible se situant en dessous de 5 000 µg/g, préférablement en dessous de 3 000 pg/g.
  4. Cible selon au moins l'une quelconque des revendications précédentes, la proportion d'éléments dotés d'un travail d'extraction supérieur ou égal à 4,5 eV dans la cible étant inférieure à 10 % at.
  5. Cible selon au moins l'une quelconque des revendications précédentes, les composés céramiques étant choisis dans le groupe des borures et/ou des carbures et/ou des nitrures et/ou des siliciures.
  6. Cible selon au moins l'une quelconque des revendications précédentes, l'élément de dopage étant le cérium et étant présent en tant que composé céramique sous forme de disiliciure de cérium.
  7. Procédé de préparation par métallurgie des poudres d'une cible selon l'une quelconque des revendications précédentes, qui est destinée à l'utilisation dans un processus de dépôt physique en phase vapeur, dans lequel, pour la préparation d'un lot de poudres, des éléments de dopage sont introduits dans une poudre métallique et le lot de poudres est densifié, et la poudre métallique étant choisie dans le groupe constitué par un matériau à base d'aluminium et/ou un matériau à base de titane, caractérisé en ce que les éléments de dopage sont introduits en tant qu'ingrédients de composés céramiques dans la poudre métallique et en ce que des éléments du groupe des lanthanoïdes : La, Ce, Nd, Sm et Eu sont utilisés en tant qu'éléments de dopage, les composés céramiques contenant les éléments de dopage étant utilisés en une concentration supérieure à 1 % en moles jusqu'à inférieure ou égale à 25 % en moles, de préférence inférieure ou égale à 10 % en moles à chaque fois par rapport au lot de poudres.
  8. Utilisation d'une cible selon au moins l'une quelconque des revendications 1 à 6 ou préparée selon la revendication 7 dans un processus de dépôt physique en phase vapeur.
EP18706710.3A 2017-02-28 2018-02-19 Cible de pulvérisation et procédé de production d'une cible de pulvérisation Active EP3589773B1 (fr)

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ATGM46/2017U AT15596U1 (de) 2017-02-28 2017-02-28 Sputtertarget und Verfahren zur Herstellung eines Sputtertargets
PCT/EP2018/054041 WO2018158101A1 (fr) 2017-02-28 2018-02-19 Cible de pulvérisation et procédé de production d'une cible de pulvérisation

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CN111188016B (zh) * 2019-12-30 2023-07-04 苏州六九新材料科技有限公司 一种高性能CrAlSiX合金靶材及其制备方法
CN111057905B (zh) * 2020-01-13 2022-03-04 西安理工大学 一种粉末冶金制备铌钛合金的方法
CN112063893B (zh) * 2020-09-29 2021-12-10 中国科学院金属研究所 一种高热稳定性等轴纳米晶Ti6Al4V-Fe合金及其制备方法
CN112962069B (zh) * 2021-02-02 2023-04-28 长沙淮石新材料科技有限公司 一种含金属间化合物的铝合金靶材及其制备方法
CN114727467B (zh) * 2022-04-13 2023-06-16 中国科学技术大学 一种组合式直热六硼化镧等离子体源
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US11767587B2 (en) 2023-09-26
US20190368029A1 (en) 2019-12-05
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JP2020511598A (ja) 2020-04-16
JP7198211B2 (ja) 2022-12-28
CN110536974B (zh) 2022-03-04
AT15596U1 (de) 2018-03-15
WO2018158101A1 (fr) 2018-09-07
CN110536974A (zh) 2019-12-03

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